Larimax. Residual Gas Analysers and Gas Analysis Systems. Index. Low Cost PC Controlled RGA PC Controlled RGA for gas analysis

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1 Larimax Residual Gas Analysers and Gas Analysis Systems P.C. Controlled RGA s AX200 AX600 DQC2000 RX200 HPQ Series Software Stand Alone RGA Dataquad Index Low Cost PC Controlled RGA PC Controlled RGA for gas analysis PC Controlled RGA for gas analysis Isolated Electronics for radiation environment Large High Power Quadrupole. For PC Controlled RGA s Stand Alone RGA Inlet systems Inlet types High Pressure Semiconductor Description of different inlet types Inlets for sampling from High Pressure. Dual Inlet for Sputtering Systems. Gas Analysis Systems Compass TGA1 Bio-Quad Options Ion Source Options Filaments. Filament Information. Systems for General Gas Analysis Environmental and Trace Gas Analysis System for fermentation.

2 Larimax AX200 Quadrupole Mass Spectrometer

3 The AX-200 Residual Gas Analyser *Very Compact RGA *Low Power requirements *Comprehensive Software *Lowest Cost RGA available *Twin Filament *Wide Range of Options *High Pressure Facility *Sub ppm Detection The AX-200 mass spectrometer system can be configured to meet most gas analysis and process monitoring applications. With mass ranges up to 300amu and a choice of detector systems the AX-200 may be supplied as an add on to an existing vacuum system or as a complete stand alone unit with integrated vacuum and inlet system. The AX-200 uses a PC Computer as its system controller and its operating software is written in a high level language to simplify updating and to allow easy customising to meet specific process requirements. The user friendly software operating under 'Windows 95/98' or NT make the AX-200 easy to use in all RGA and gas analysis applications. The Analyser. The quadrupole analyser is available with a choice of ion sources and detection systems. The standard ion source is a radially symmetrical design fitted with twin filaments and suits most applications. The standard filaments are tungsten but thoria coated iridium are available if required. The Electronics Unit. This compact unit contains the complete quadrupole electronics and plugs directly onto the analyser. Communication with the PC Computer is via the RS232. The unit has a performance and features only found on more expensive RGA s, and yet its small size and low cost is achieved by the use of the very latest electronic techniques.

4 Technical Data Mass Range 1-100, (Specials 1-45 & 1-15) Resolution Minimum detectable partial pressure Minimum detectable total pressure 10% valley between equal peaks 2 x 10-11mBar Faraday. 5 x 10-14mBar SEM. 1 x mbar. Maximum operating pressure 1 x 10-3 mbar Faraday. 1 x 10-5 mbar SEM. Electron energy Ion energy. Emission (Normal Mode/High Pressure Mode) Bakeout Temperature R.F. frequency R.F. amplitude. Rod diameter Rod length 70eV 6eV. 1 ma./100ua 250 C recommended 350 C maximum. 1.84Mhz std. (1.6Mhz, 2.5Mhz, 3Mhz. 4.9Mhz) 800V p/p at maximum mass 6.35 mm. 100 mm. Std. Power requirements volts 16 watts. Baud Rate 600 to 38,400 Dynamic Data Exchange (DDE) Software O/P 2nd RS232 Software O/P Software Features P.C. Computer required. Data Transfer to other applications Data transfer to Host Computer (Option) Refer to separate leaflet. IBM Compatible with windows 95/NT4 or above Dimensions in mm. Analyser 125mm 88mm 77mm 120mm* 153mm *Faraday versions = 120mm Channeltron version = 125mm Electronic Unit Order Information. Complete Instruments: AX200/100F 100amu with Faraday Detector. AX200/200F 200amu with Faraday Detector. AX200/ 100S 100amu with Dual Detector. AX200/ 200S 200amu with Dual Detector. AX200/24V 24 VDC Reg. Power Supply. Spare Analyser Heads. AX200/200F Analyser with Faraday Collector AX200/200S Analyser with dual Detector Spare Filaments. AX100FW Pack of 4 Tungsten SM100FT Pack of 2 Thoria coated Iridium. Anglo Scientific Instruments. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. U.K. Tel: +44 (0) Fax: +44 (0) sales@a-s-i.demon.co.uk Return to Index

5 Larimax AX600 Quadrupole Mass Spectrometer

6 The AX-600 Residual Gas Analyser *Very Compact RGA *Low Power requirements *Comprehensive Software *Lowest Cost RGA available *Twin Filament *Wide Range of Options *High Pressure Facility *Sub ppm Detection The AX-600 mass spectrometer system can be configured to meet most gas analysis and process monitoring applications. With mass ranges up to 500amu and a choice of detector systems the AX-600 may be supplied as an add on to an existing vacuum system or as a complete stand alone unit with integrated vacuum and inlet system. The AX-600 uses a PC Computer as its system controller and its operating software is written in a high level language to simplify updating and to allow easy customising to meet specific process requirements. The user friendly software operating under 'Windows 98' / NT or above, make the AX-200 easy to use in all RGA and gas analysis applications. The Analyser. The quadrupole analyser is available with a choice of ion sources, mass filters and detection systems. The standard ion source is a radially symmetrical design fitted with twin filaments and suits most applications. The standard filaments are tungsten but thoria coated iridium are available if required. The standard mass filter is a 100mm long with 6.35mm diameter cylindrical rods. Hyperbolic mass filter with pre and post filters are available for high mass applications or when the best available performance is required. The detector is a combined Faraday cup and channeltron detector. A Faraday detector only is available if required. The Electronics Unit. This compact unit contains the complete quadrupole electronics and plugs directly onto the analyser. Communication with the PC Computer is via the RS232. The unit has a performance and features only found on more expensive RGA s, and yet its small size and low cost is achieved by the use of the very latest electronic techniques.

7 Ion Source Options. Open Ion Source. (Fitted as Standard) This ion source is used for residual gas analysis and simple gas analysis applications. Axial Beam Ion Source. This ion source is specifically for analysing either molecular beams or ion beams from an external source. The ion source has a low profile with side mounted filaments so that the source can be positioned close to the exit hole of a source of ions or molecular beam that is in line with the axis of the quadrupole. Cross Beam Ion Source. This source is for molecular beams that enter the ion source at right angles to the quadrupole. A clear aperture of 3,5mm avoids contact with the molecular beam. This source is normally used in applications where condensable vapors may be present within the molecular beam that could contaminate the quadrupole filter. Mass Filter Options. Single Mass Filter. (Fitted as Standard) A Low cost single stage mass filter using cylindrical rods for low mass applications. Hyperbolic Mass Filter. A Monolithic Mass filter constructed from low expansion Borosilicate glass. Gold plated electrodes are deposited onto the precision ground hyperbolic surfaces. This filter offers improved sensitivity, resolution and abundance sensitivity. Dual & Triple filters. These are available based on the hyperbolic mass filters, and are normally chosen for high mass applications or when the highest performance is required. Detector Options. Faraday Only. A Faraday plate detector for ion collection. Used mainly for higher pressure applications when greater ion currents are available for collection. Dual Faraday/Channeltron. (Fitted as Standard) The channeltron (SEM) provides a high level of amplification of the ion beam and therefore provides detection of much lower ion currents. Pulse Counting. Provides the ultimate in detection by counting individual ions arriving at the detector.. Normally used in trace gas analysis applications where the lowest level of detection is required. A special version of the electronics is available that includes a counting preamplifier, system clock, counter, and interface for transferring the accumulated ion count to the quadrupole software for display. Systems. Vacuum Systems. Bench Top or Floor standing Turbo molecular pumped vacuum systems are available. Housing for the mass spectrometer and inlet port for coupling the inlet system are included. Options include high and low vacuum gauges, interlocking to provide fail safe operation. Inlet Systems. A wide range of on-line and off-line gas inlet systems are available to suit your gas analysis application.

8 Technical Data AX600. Mass Range Options Resolution* Minimum detectable partial pressure 1-100, 1-200, 1-300, (Others available) 5% valley between equal peaks* x 10 mbar Faraday. 2 x 10 mbar SEM. Minimum detectable total pressure x 10 mbar. Maximum operating pressure -4 1 x 10 mbar Faraday x 10 mbar SEM. Electron energy Ion energy. Emission Bakeout Temperature eV 1-20eV. 10uA -2mA. 250 C recommended 350 C maximum. R.F. frequency 1.6Mhz, 1.84Mhz, 2.5Mhz, 3Mhz. 4.9Mhz R.F. amplitude. Rod diameter Rod length 1200V p/p at maximum mass 6.35 mm cylindrical. (Hyperbolic available) 100 mm. std. (125 mm. for 300 amu.) Power requirements volts watts. Baud Rate 600 to 56,600 Mass Filter Options. Ion Source Options. Further Software Features P.C. Computer required. Hyperbolic, Dual, Triple. Open, Axial Beam, Cross Beam, Nibtron. Refer to separate leaflet. IBM Compatible with windows 98/NT4 or above *Resolution based on standard 100mm cylindrical rod mass filter. Dimensions in mm. The housing for the analyser should have an internal diameter of 35mm or more to give adequate clearance. Analyser length from flange face:= * Faraday versions = 120mm * Channeltron version = 125mm * 300amu and above = 150mm Analyser 120mm* 135mm 98mm 180mm Electronic Unit 86mm Order Information. Complete Instruments: AX600/ 100S 100amu with Dual Detector. AX600/ 200S 200amu with Dual Detector. AX600/300S 300amu with Dual Detector. AX600/400S 400amu with Dual Detector. AX600/500S 500amu with Dual Detector. Spare Analyser Heads. AX/100S Analyser with dual Detector Spare Filaments. AX100FW Pack of 4 Tungsten SM100FT Pack of 2 Thoria coated Iridium. Larimax/ASI. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. U.K. Tel: +44 (0) Fax: +44 (0) sales@a-s-i.demon.co.uk Return to Index

9 Larimax DQC2000 QUADRUPOLE MASS SPECTROMETER

10 The DQC2000 Residual Gas Analyser The DQC2000 series of computer integrated mass spectrometer systems can be configured to meet most gas analysis and process monitoring applications. With mass ranges upto 300amu and a choice of detector systems the DQC2000 may be supplied as an "add on" to an existing vacuum system or as a complete stand alone unit with integrated vacuum and inlet system. The DQC2000 uses a PC Computer as its system controller and its operating software is writen in a high level language to simplify updateing and to allow easy customising to meet specific process requirements. The user friendly software operating under 'Windows 95/98' make the DQC2000 easy to use in all RGA and gas analysis applications. The Analyser. The quadrupole analyser is available with a choice of ion sources, mass filters and detection systems. The standard ion source is a radially symmetrical design fitted with twin filaments and suits most applications. The standard filaments are tungsten but thoria coated iridium are available if required. The R.F. Head/Pre-amp. This compact unit contains the pre-amplifier and RF generation/control electronics and plugs directly onto the analyser to prevent signal degradation. The standard cable length is 2 metres but extension cables up to 100 metres can be supplied if required. The Computer Interface Card. This special interface card is manufactured by Larimax and is designed to fit into a spare full length slot of a PC type computer. The Control Unit. The control unit contains the main power supplies for the instrument including the emission and filament control circuits which are housed in a 2U high 19 inch rack module Order Information. Complete Instruments: DQC100F 100amu R.G.A. with Faraday Detector. DQC100M 100amu R.G.A. with Dual Detector. DQC200M 200amu R.G.A. with Dual Detector. DQC300M 300amu R.G.A. with Dual Detector. Spare Analyser Heads. ASI200F Analyser with Faraday Collector ASI200M Analyser with dual Detector ASI300M Analyser with Dual Detector ( 300amu.) Spare Filaments. SM100FW Pack of 4 Tungsten SM100FT Pack of 2 Thoria coated Iridium. High Pressure Operation. A unique feature of the DQC2000 is that it has a built in high pressure mode.when this mode is selected source parameters are changed, the amplifier gain is automatically changed to maintain the correct pressure scale. The maximum operating pressure is now increased -3 to 10 mbar. In the high pressure mode the analyser and the filament life are greatly extended. Gas Analysis Systems. Larimax also specialise in the manufacture of vacuum systems and a wide range of inlet systems and are able to offer complete gas analysis systems for different applications.

11 Technical Data Mass Range 1-15, 1-50, 1-100, 1-200, Resolution Minimum detectable partial pressure Minimum detectable total pressure 10% valley between equal peaks 2 x 10-11mBar Faraday. 2 x 10-14mBar SEM. 1 x mbar. Maximum operating pressure 1 x 10-3 mbar Faraday. 1 x 10-5 mbar SEM. Electron energy Ion energy Emission (Normal Mode) Bakeout Temperature R.F. frequency R.F. amplitude. Rod diameter Rod length Power requirements Software specifications P.C. Computer required. 70eV 6eV. 1 ma. 250 C recommended 350 C maximum. 1.84Mhz std. (1.6Mhz, 2.5Mhz, 3Mhz. 4.9Mhz) 800V p/p at maximum mass 6.35 mm. 100 mm. std. (125 mm. for 300 amu.) 105/115/220/240 volts 50/60 Hz 50 watts. Refer to separate leaflet. IBM Compatible with Windows installed Dimensions in mm. Control unit Analyser 100mm 50mm 88mm 120mm 195mm 230mm 482mm RF Head Represented by Larimax/ASI.. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. Tel: +44 (0) Fax: +44 (0) website sales@a-s-i.demon.co.uk Return to Index

12 Larimax RQ200 QUADRUPOLE MASS SPECTROMETER

13 The RQ200 Residual Gas Analyser The RQ200 series of computer integrated mass spectrometer system has been designed for radiation environments where it is necessary for the electronics to be separated a long distance from the quadrupole sensor head to avoid damage to sensitive electronic components.. The instrument is fitted with a Channeltron detector as standard and is available with a choice of mass range. The RQ200 uses a PC Computer as its system controller and its operating software is written in a high level language to simplify updating and to allow easy customising to meet specific user requirements. The user friendly software operating under 'Windows ' make the RQ200 easy to use in all RGA applications. The Control Unit. The control unit contains all the electronic circuits for the quadrupole including the emission and filament control circuits, R.F Generator, main amplifier and interface circuits. These are housed in a 3U high 19 inch rack module. All the electronics are on plug in circuit cards to simplify for easy maintenance and servicing. Connection to the computer is via RS232 cable or fibre optic link. The R.F. Matching unit. This compact unit, free of active components, plugs directly onto the analyser. It allows the electronics to be separated from the analyser by up to 20 metres with very little R.F. power loss in the cables. This elliminates the need for high R.F. Powers greatly improving reliability and stability. The Analyser. The quadrupole analyser is fitted with an open ion source designed for UHV application. It is a radially symmetrical design fitted with twin filaments. The standard filaments are tungsten but thoria coated iridium are available if required. A Channeltron electron multiplier is fitted as standard.

14 Technical Data Mass Range 1-100, 1-200, Resolution Minimum detectable partial pressure Minimum detectable total pressure 10% valley between equal peaks 2 x 10-14mBar SEM. 1 x mbar. Maximum operating pressure 1 x 10-4 mbar Faraday. 1 x 10-5 mbar SEM. Electron energy Variable eV Ion energy Emission Variable Variable 1-25eV. 50uA- 1 ma. Bakeout Temperature R.F. frequency R.F. amplitude. Rod diameter Rod length Power requirements Separation of quadrupole sensor from electronics P.C. Computer required. 250 C recommended 350 C maximum. 2.0MHz/ 2.5Mhz 980V p/p at maximum mass 6.35 mm. 100 mm / VAC 40Watts Up to 20 metres IBM Compatible with Windows installed Dimensions in mm. 85mm 48mm 70mm 133mm 125mm Analyser 483mm Electronics Unit Software features Refer to software leaflet for details Larimax/ASI. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. Tel: +44 (0) website http// sales@a-s-i.demon.co.uk Return to Index

15 A.S.I The NEW Mk 4 HPQ Series QUADRUPOLE MASS SPECTROMETER

16 The New Mk4 HPQ-Series Quadrupole system. The new HPQ series of quadrupole mass spectrometers are designed for the more demanding applications not easily satisfied by small RGA type quadrupoles. These applications include process monitoring and control, precision gas analysis, trace detection down to ppb levels, molecular beam applications and as a general high performance analysis tool for research. Designed by ASI, they are IBM compatible PC controlled units with extensive standard software including with added application specific software where required. To cater for all applications, each model is available in 2 variants standard with fixed operational parameters and E versions with computer contriol of electron energy, emission current, and ion energy. The user friendly software operating under 'Windows make the HPQ easy to use in all RGA and gas analysis applications. HARDWARE DESCRIPTION. The Analyser. The quadrupole analyser is available with a choice of ion sources, mass filters and detection systems. The standard ion source is a radially symmetrical design fitted with twin filaments and suits most applications. The standard filaments are tungsten but thoria coated iridium are available if required. The R.F. Head/Pre-amp. The Pre-amp unit contains plugs directly onto the analyser to prevent signal degradation. The new Mk4 R.F Generator is a small compact unit that is positioned close to the analyser. This then connects to the main control unit through a 2 metre cable, but extension cables up to 100 metres can be supplied if required. The Control Unit. The control unit contains the main power supplies for the instrument including the emission and filament control circuits which are housed in a 3U high 19 inch rack module. All the electronics are on plug in circuit cards to simplify servicing. An interface card built into the control unit connects to a PC Computer via the RS232 and Gas Analysis Systems. A.S.I. also specialise in the manufacture of vacuum systems and a range of different inlet systems and are able to offer complete gas analysis systems for a wide range of applications. Other Q.M.S..Instruments:- DQC2000 PC Controlled low cost mass spectrometer for RGA and gas analysis. Spectramass DATAQUAD: Stand alone instrument with built in monitor and switch panel. AX200: PC Controlled RGA which interfaces the computer via RS232.

17 Technical Data Mass Range 1-50, 1-100, 1-200, 1-300, Resolution Minimum detectable partial pressure Minimum detectable total pressure 10% valley between equal peaks 2 x 10-11mBar Faraday. 2 x 10-14mBar SEM. 1 x mbar. Maximum operating pressure 1 x 10-4 mbar Faraday. 1 x 10-5 mbar SEM. Electron energy Ion energy Emission Bakeout Temperature R.F. frequency R.F. amplitude. Rod diameter Rod length Power requirements Software specifications P.C. Computer required. 70eV (10-100eV on E Model) 6eV. (2-25eV on E Model) 1 ma. (10uA -5mAonEModel) 250 C recommended 350 C maximum. 1.6Mhz, 1.84Mhz 2.5Mhz, 3Mhz. 4.9Mhz 2000V p/p at maximum mass 6.35 mm. (10.0mm option) 15 cm. std. (20 cm. for 1cm dia rods) 105/115/220/240 volts 50/60 Hz 150 watts. Refer to separate leaflet. IBM Compatible Dimensions in mm. 150mm Control unit Analyser 102/152mm 132mm mm 482mm 305mm 130mm 270mm RF Head 250mm Represented by Anglo Scientific Instruments. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. Tel: +44 (0) Fax: website sales@a-s-i.demon.co.uk Return to Index

18 Larimax Quadrupole Operating Software

19 Quadrupole Operating Software. The new 'Windows' software for the Larimax mass spectrometers has been designed to be 'user friendly' quick to operate and very simple to learn and use. Main Display Modes Bar-Graph Mode In Bar graph mode a region of the mass spectrum is measured at integral values of mass number and the resulting partial pressures are plotted against mass number in a bar-graph format. The first mass and scan width of the display can be quickley changed by the adjustment of scroll bars and the instrument gain range can be quickly changed from the gain display panel DATE/TIME is updated at the start of each scan, and stored if a spectra save is implemented. TOTAL ON/OFF Select ON and Total Pressure will be read and updated at the end of each scan PRESSURE SCALE Choice of mbar/torr/pascal GAIN PANEL UP/DOWN buttons increment the gain AUTO button selects auto gain FIRST MASS & SCAN WIDTH Scroll bars. A simple and quick way to set the start and finish masses of the scan Split Screen Library Search Mode In Split screen mode the graphics area is divided into 2 parts. The lower part contains the normal online spectra. The Upper part displays the library spectra and search panel. The library contains common residuals and semiconductor gases. Search Panel. Allows user input of search mass and search type with display of search results and compound names. Buttons enable scanning of found spectra. Stored Library Spectra displayed on upper half of screen Normal online Bar Graph Spectra displayed on lower half of screen First Mass and Scan Width controls are common to both displays to maintain mass alignment

20 Channel Mode The Channel and Trend modes are identically operationally but differ in the way that recorded data is presented. In both cases the mass spectrometer makes measurements of partial pressure at up to 16 mass numbers using previously defined gain ranges and detectors. Channel Table. One Column for each channel peak, and 5 rows for peak data. To change the data in either of the first 4 rows simply click on the data that you wish to change. The box will become highlighted and a control will appear on the Change Data panel above. Now adjust the control to change the data. Information/Message Display box. UP/Down buttons to change the number of channels being Scanned and displayed. Any number between 1 and 16 can be selected. Mass number being read by mass spectrometer Trend mode shows the same peak information as channel mode except the peak heights are plotted against time. Therefore all controls including the Channel Grid Table will remain the same in both modes. Trend and Leak Detect Analogue Display This display option allows the partial pressures of upto 16 masses to be plotted against time. The plot interval can be selected and each mass is depicted as a different coloured line. The leak detect mode is a single channel version with the default mass 4 selected for helium. This is mainly used for checking on the analyser condition. It allows the peak shape and resolution of the analyser to be monitored and also simplifies the checking of mass alignment. AUTO-RUN. If Auto-Run has been selected the display will change to a table format. Filaments will switch on automatically. There will be a short delay whilst the filaments out-gas total pressure will be measured and then the instrument will start scanning over the first 100 amu. At the end of a scan the software will select the 8 largest peaks in the spectrum and display these in order on the table. The mass, gas and percentage for each gas will be indicated. The software will continue to monitor these major peaks, and comments will appear giving vacuum diagnosis, conditions, vacuum problems and how the vacuum conditions are changing. This auto-run facility is mainly for the system user, who uses the RGA as a diagnostic tool and problem solver. All by the pressing of a single button. At the bottom of this display are 3 buttons. One which closes this operating mode and returns the user to the main display modes, the second allows the whole process to start again and the third button takes the user direct to leak detect mode.

21 TOP TOOL BAR. (Drop down Menus) Software control. File menue SAVE SETTINGS. Saves all the current user settings into a text file. These include first mass Scan width, gain, channel peak information, detector, etc. LOAD SETTINGS. Loads all the last saved setting information. This is also automatically loaded during bootup of the software, so the instruments returns to the same condition, and settings as it was when switched off. SAVE USER SETTINGS. Saves all the current user settings into a Named text file. Any number can be saved. Useful for different operators, or different configurations of the Software. LOAD USER SETTINGS. Loads all the last saved setting information from a Named user settings file. SAVE SPECTRA. Saves the current spectra at the end of scan into a text file along with all instrument parameters and date /time information. RETRIEVE SPECTRA. Retrieves spectra from file. The software reconstructs and displays the spectra and all instrument settings at the time the spectra was saved. DATALOG. Saves Channel/Trend Spectra data for up to 16 peaks into a text file. This data can be printed, displayed or transferred to a spreadsheet for further processing. PRINT. Prints hard copy of the current displayed spectra in graphical form. EXIT. Automatic shut down of instrument and software. Display Mode menue Selects one of the 5 main operating modes. Bar Graph, Analogue, Channel, Trend and Leak Detect. System menue. Selection of set up menus for changing serial port settings and engineers panels for testing hardware and configuring the software to the hardware in use. Options menue. Allows leak mass to be changed, mass calibration, and High Pressure mode to be selected. Scan menue. Selects different fast scanning options, and single shot/normal scan mode. Background Subtract. Menu options to allow the background spectra to be stored and the later subtracted from the current spectra after gas has been admitted to the system. Library Mode. Allows Split Screen Mode to be selected with a search facility to display Library spectra above the current spectra. (Bar-Graph Mode only). Help. Provides online help with descriptions of the main software features and controls. BOTTOM TOOL BAR Mass Spectrometer Control. Status. Displays current status of the filament and emission, and will display any warning messages should the filament fail. Filament Control Panel. Allows filaments to be selected ON/OFF with single button operation. Detector Control Panel. FARADAY button. Selects Faraday plate ion detector mode. S.E.M. Button. Switches on the high voltage to the Secondary electron multiplier. (Dual detector instruments only). CAL. Button. Automatically calibrates the electron multiplier to a pre-set gain. A Calibration panel indicates progress and gain achieved at completion. Scan Control Panel. START button. Starts the instrument mass scan. Either from the first mass, first channel, or last stop position. STOP button. Stops the current scan in its present mass/channel position. RESET button. Resets the mass scan to first mass or channel 1, in either start or stop mode. Precision Code. UP/DOWN buttons. Gives selection of 8 precision codes. Higher code number increases the number of peak readings, integrations, and therfore gives give more accurate and reproducible results. Peak Width. Up/Down buttons. Changes the amount of the peak that is scanned. 0% represents a single plotting point. 100% corresponds to 16 plotting points. Larimax is a strongly design/development orientated company and additional Features and improvements will appear from time to time. Therefore Larimax reserve the right to change specifications and features without notice. Users of Larimax instruments will automatically receive free upgrades as and when they become available. E & OE. Larimax/ASI. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. U.K. Tel: +44 (0) Fax: +44 (0) sales@a-s-i.demon.co.uk Return to Index

22 Larimax The Spectramass DATAQUAD

23 The 'DATAQUAD' Residual Gas Analyser The Dataquad RGA is a complete 'Stand Alone' RGA system with its own mictroprocessor electronics. With a dedicated keyboard, monochrome monitor and extensive software, Dataquad offers the user exceptional performance at low cost. All Dataquads are supplied with Datapacks 1, 2 and 3 providing the main operating modes of Bar Graph, Peak Select (Channel and Trend), Analogue and Leak Detect with facilities such as logarithmic or linear display, backgrounds, library and split spectrum display. RS232 and centronics ports are standard. A separate software package is available to control and display the Dataquad from a PC Computer, which offers many additional facilities including datalogging and data recall/review. Refer to supplementary leaflet for further information. The Analyser. The quadrupole analyser is available with a choice of ion sources, mass filters and detection systems. The standard ion source is a radially symmetrical design fitted with twin filaments and suits most applications. The standard filaments are tungsten but thoria coated iridium are available if required. The R.F. Head/Pre-amp. This compact unit contains the pre-amplifier and RF generation/control electronics and plugs directly onto the analyser to prevent signal degradation. The standard cable length is 2 metres but extension cables up to 100 metres can be supplied if required. The Control Unit. The control unit contains all the main power supplies, microprocessor and interface electronics mounted on 3 plug-in easily replaceable circuit cards. The unit also contains a 9" display monitor and a dedicated membrane key panel to provide a complete 'stand alone' RGA system housed in a 5U high 19 inch rack module. Software description BarGraph Mode This display mode of mass versus partial pressure gives a bar representation (spectrum histogram) of the peaks detected during a scan. The operator can select the first mass, display scan, precision code, mass identify cursor and full span. There are 6 precision codes giving a choice of speed/accuracy combinations, and the gain may be controlled manually or automatically by the microprocessor. The total pressure can be enabled/disabled as a menue option and when enabled, the value is displayed on the top right hand corner of the VDU. Peak Select. The Peak Select mode offers an alternative to scanning all the masses sequentially and enables up to 16 masses to be monitored in table format and upto 8 masses in histogram form. The two modes being toggled by the Table/Graph key. The operator has control over mass, gain (or auto), detector and alarm levels for each individual channel making Peak Select a powerful aid to vacuum analysis. When alarms are activated, signals are available as TTL levels on the rear panel, for process monitoring applications.

24 Index (Menue Options). The Dataquad can be operated in the modes mentioned above without entering the index. There are however some useful additional functions available which are accessed by first entering Index and then moving the cursor to the function required and making the selection by pressing the enter key. Trend Analysis. This display option allows the partial pressures of upto 8 masses to be plotted against time. The plot interval can be selected from i second to 10 minutes and the values may be shown on the VDU as numerical entries in 8 columns or as horizontal bars in each mass column, the length of which depends on the partial pressure. The table/graph key is used to toggle between the two alternative display formats. Analogue Display. This is mainly used for checking on the analyser condition. It allows the peak shape and resolution of the analyser to be monitored and also simplifies the checking of mass alignment. Diagnostics Automatic check of main power supplies. Out of specification supplies are indicated by a fail code message. Details are in the operators manual. Protect. User may select Total and/or partial pressure trip. Total pressure trip operates in bar graph mode only when reading reaches 10 x 10-6 torr. Partial pressure trip operates in any scanning mode when a peak exceeds full scale. Both trips switch off the filament. Timed Printout. The operator may select via the print key either 'single' or 'timed' print. In timed mode, the time interval set (max 99 mins) is activated to provide a printout of screen display after the interval has elapsed. Background Store. Allows the user to store any one mass spectrum from the Bar graph mode. Background Display Recalls and displays the stored spectrum. Scanning restarted by pressing the STOP/RUN key (or a function key). Background Subtract. Subtracts the store spectrum from the 'on-line' spectrum in bar graph mode. Degas. To degas Ion Source with user setting of degas time. Split Screen When selected with the bar graph mode, the screen display area is split into two sets of axes. The top set shows the current mass spectrum, whilst the lower displays the mass spectr library with the facility to step through the individual spectra for comparison purposes. Alternatively using the background display key, any of the four user stored spectra can be reviewed. An autosearch is provided allowing the user to select a peak in the current bar graph spectrum which is then compared to the mass spectra library, and any matches are sequentially displayed on the screen Multiplier Calibration. Measures mass 28 with the faraday detector, switches on the multiplier and adjust the gain to a factor of 100. Reset. Returns programmed values of each mode to the factory set values. Pressing a second time returns to user values. Max Peaks. Operates from any mode. Bar graph is automatically selected and the 8 largest peaks are located, loaded sequentially into the peak select programme and then Dataquad then runs in Peak Select mode. Auto-Run. On activation, a confirmation that vacuum is O.K. is requested. The filament is then switched on and a 15 minute warm up time will elapse. Then the diagnostics routine is activated followed by operation in the last used mode. Filament 1 and 2. The keys select filament 1 or filament 2, a second press on the key switching the filament off. Leak Detect. Sets the quadrupole to mass 4 and displays a graph of mass 4 signal versus time. ENABLE/DISABLE switches off the audio tone. Manual control of gain is available. The mass may be programmed and is remembered for subsequent selection of this mode. Print. Provides a single printout at the end of the scan onto a printer. SEM. (Dual Detector only) Selects the electron multiplier with gain of 100. Note that Total Mode is still provided in this mode, when enabled from the index. 3-Decade Display. This display format is available in bar graph mode, plotting peak heights over any 3 consecutive decades of gain in a logarithmic type display. With this dynamic range of 1000 to 1, large and small peaks may be displayed on the same axis.

25 Technical Data Mass Range 1-100, 2-200, Resolution Minimum detectable partial pressure Minimum detectable total pressure 10% valley between equal peaks 2 x 10-11mBar Faraday. 2 x 10-13mBar SEM. 1 x mbar. Maximum operating pressure 1 x 10-4 mbar Faraday. 1 x 10-5 mbar SEM. Electron energy Ion energy Emission Bakeout Temperature R.F. frequency R.F. amplitude. Rod diameter Rod length Power requirements Software specifications 70eV 6eV. 1 ma. 250 C recommended 350 C maximum. 1.84Mhz std. 800V p/p at maximum mass 6.35 mm. 100 mm. std. 105/115/220/240 volts 50/60 Hz 50 watts. Refer to separate leaflet. Integral VDU Order Information. Complete Instruments: DAQ100DXS 100amu R.G.A. with Faraday Detector. DAQ100DXM 100amu R.G.A. with Dual Detector. DAQ200DXS 200amu R.G.A. with Faraday Detector. DAQ200DXM 200amu R.G.A. with Dual Detector. 9" monochrome Dimensions in mm. Control unit Additional Analyser Heads. ASI200F Analyser with Faraday Collector ASI200M Analyser with dual Detector Spare Filaments. SM100FW Pack of 4 Tungsten SM100FT Pack of 2 Thoria coated Iridium. Represented by: Analyser 482mm 100mm 50mm 311mm 239mm 120mm 195mm RF Head E & O.E. Larimax/ASI.. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. Tel: +44 (0) Fax: +44 (0) Website sales@a-s-i.demon.co.uk Return to Index

26 Larimax. Inlet Systems for Quadrupole Mass Spectrometry. -4 Quadrupole Mass Spectrometers, because of their nature, require an operating vacuum of 10 mbar -4 or better. However most processes which need monitoring occur at a pressure in excess of 10 mbar. It is necessary therefore to have some form of interface between the mass spectrometer and the process vessel. These interfaces are called Inlet Systems and the type required is dependent upon the application. Capillary Inlet This system is a form of continuous gas sampling, and may be used across a pressure range of 10-4 mbar to atmospheric pressure (1000 mbar). It consists of a narrow tube which connects the sampling point to the mass spectrometer vacuum system. The length and internal diameter of the tube have to be selected according to the pressure at which the sample is taken. The disadvantage of this system is that at higher sampling pressures ( above 100 mbar) the response time becomes very long (of the order of a few minutes ) due to the length of the tube. This can be overcome by a bypass type inlet system. Capillary Inlet with bypass. This type of inlet system is better suited to sampling over a pressure range from 100 mbar to well above atmospheric pressure. The operating principle is that a capillary tube is connected to a T-piece which is attached to a rotary pump. To the third arm is fitted a molecular flow leak or leak valve. Gas is drawn along the capillary by the rotary pump and a small portion of the gas which flows through the T- piece, passes across the leak and into the mass spectrometer. This inlet requires a gas flow of approximately 20 ml min and achieves a response time of better than 80ms. Heated capillary inlets are also available, which improve response time, reduce memory effects and reduce condensation within the capillary. A crimp at the sample end to restrict the sample gas flow and a throttle valve on the bypass pump will allow much smaller sampling rates and still maintain good response times. Sample Sample gas above mbar Figure 2 Capillary Throttle Valve (Optional) Capillary Rotary Pump Figure 1 Mass Spectrometer Vacuum System Leak Mass Spectrometer Leak Valve Inlets. A good, continuous sampling, leak valve can provide the flexibility to sample across a range of 10-5 torr to well above atmospheric pressure. The operating principle is the precise control of a knife edge biting into a surface. The knife edge position is controlled by a fine screw operating mechanism with a calibrated dial so that a particular leak rate may be reproducibly set. The main disadvantage of this method of gas sampling is that fractionation of the gas occurs across the valve seat and the degree of fractionation depends on the leak rate setting. It therefore makes calibration of this inlet difficult. Response times when sampling from higher pressures may also be long unless attention is paid to producing a continuous gas flow across the valve seat. The inlet is available either as a general purpose, polymer sealed valve or as an all metal precision valve.

27 Membrane Inlet. A membrane system consists of a tube terminating in a special semi-permeable membrane stretched over a grid. The type of membrane selected is determined by the application and the components of interest in the sample, as the membrane can exert considerable selectivity. Perhaps the most common types of membrane material employed are Teflon and silicone rubber. Teflon is normally used for disolved gases in organic liquids. Silicone is highly permeable to oxygen and can be used for the monitoring of organic compounds in situ. The major application of this inlet is in detecting inpurities in process gas, environmental monitoring and sample enrichment, particularly of organic materials, where the low levels would fall below the normal detection limit of the mass spectrometer. system. Membrane Exhaust Carrier Gas In Membrane St/St Tube Figure 3. Mass Spectrometer Process Gas Inlet of Mass Spectrometer Liquid Batch Inlet System. Continuous sampling techniques are satisfactory provided the mass spectrometer can be sited close to the sampling point. As this is not always possible a sample must be collected in a suitable vessel and transferred to the mass spectrometer. Introducing the gas into a vacuum system requires a batch inlet Batch inlets can be specially designed to meet particular applications but they generally consist of a reservoir which is connected by valves to a vacuum system. The sample can be introduced through a septum port (if the sample is in a gas sysringe) or through a valve port (if contained in a glass or metal collection flask). Options might include the ability to purge the reservoir with inert gas or heat the chamber to reduce background levels between samples (especially useful if water is being measured). Another useful option is the addition of a pressure gauge. Simple Batch Inlet Gauge Figure 4 V4 Sample Sample Reservoir Pumps V1 V3 V2 Mass Spectrometer Dual Inlets. Dual inlets consist of a high conductance isolation valve, and a leak valve placed in parallel across a single inlet line. The wide range in the respective conductances mean that this single system can sample from atmospheric pressure to high vacuum. This capability is particularly useful in applications such as sputtering where the pressures can alter dramatically during different stages of the process. Sputtering System Leak Valve High Conductance Figure 5. Mass Spectrometer Larimax/ASI.. 3 Devon Units, Hatchmoor Industrial Estate. Torrington, N. Devon. EX38 7HP. Tel +44 (0) Fax +44 (0) sales@a-s-i.demon.co.uk

28 Larimax Inlet Systems for High Pressure Operation -4 Quadrupole Mass Spectrometers, because of their nature, require an operating vacuum of 10 mbar or better. -4 However many processes that require monitoring occur at a pressure in excess of 10 mbar. It is necessary therefore to have some form of interface between the mass spectrometer and the process vessel. These interfaces are called Inlet Systems and the type required is dependent upon the application. Pumping Requirements As it is not possible to operate a mass spectrometer at 10-2 mbar, it is necessary to have an accessory pumping unit. This comprises the analyser fitted to a turbomolecular pump which is connected to the roughing line on the sputtering system or to a separate rotary pump.. The equipment is shown diagrammatically in figure 1. Process Vessel High Conductance Valve V1. RGA Dual Inlets. Dual inlets consist of a high conductance isolation valve, and a leak valve placed in parallel across a single inlet line (Figure 1). The wide range in the respective conductances mean that this single system can sample from atmospheric pressure to high vacuum. When used on a sputtering system the high conductance valve is opened when the sputtering system is above 10-5 mbar for leak checking and residual gas analysis. V2 is a simple leak valve. It is opened and set when the sputtering system is -4-1 between 10 mbar to 10 mbar to monitor events during the sputtering process. This capability is particularly useful in applications such as sputtering where the pressures can alter dramatically during different stages in the process. Figure 1. Process Vessel Leak ValveV2. Optional High Conductance Valve Turbo Pump RGA Rotary An alternative arrangement is shown in Figure 2. The metering valve is replaced with a fixed orifice and positioned close to the mass spectrometer ion source. The quadrupole can also be fitted with a cross beam ion source which allows gas molecules to pass through the ion source at right angles to the quadrupole axis.. In this arrangement the quadrupole analyser is mounted at right angles to the molecular gas flow. Figure 2. Orifice Turbo Pump Rotary Anglo Scientific Instruments. 3, Devon Units, Hatchmoor Industrial Estate. Torrington, N. Devon. EX38 7HP. Tel: +44 (0) Fax:- +44 (0) sales@a-s-i.demon.co.uk

29 Larimax. Semi-Conductor Industry-Use of a mass spectrometer The use of a mass spectrometer in the semiconductor industry is rapidly becoming an established technique. Two ares in particular where quadrupoles quickly repay their initial investment are Sputtering and Plasma Etching. Dual Inlets. Dual inlets consist of a high conductance isolation valve, and a leak valve placed in parallel across a single inlet line. The wide range in the respective conductances mean that this single system can sample from atmospheric pressure to high vacuum. This capability is particularly useful in applications such as sputtering where the pressures can alter dramatically during different stages in the process. Pumping Requirements As it is not possible to operate a mass spectrometer at 10-2 mbar, it is necessary to have an accessory pumping unit. This comprises the analyser fitted to a turbomolecular pump which is connected to the roughing line on the sputtering system. There are two valves fitted to allow gas from the sputtering system to flow to the mass spectrometer. Valve V1 which is a high conductance valve is opened when the sputtering system is at 10-6 mbar for leak checking and residual gas analysis. Valve V2 which is a -3-1 simple leak valve is opened and set when the sputtering system is between 10 mbar to 10 mbar to monitor events during the sputtering process. The equipment is shown diagrammatically in figure 1. Sputtering System A Leak Valve B RGA Analyser High Conductance Valve Turbo Pump Figure 1. Rotary Pump

30 SPUTTERING In this process the first stage is evacuation of the sputtering vessel to 10-6 mbar or better. At this point, the quadrupole may be used to check the quality of the vacuum, for air leaks, high background level of water, adverse hydrocarbon levels or other contaminants which may affect the sputtering process. Air leaks may quickly be cured by monitoring mass 4 with the quadrupole and probing the vessel with helium to locate the source of the leak. The following table indicates the peaks to be monitored to check for the above faults. Problem. Monitor masses. Air Leak 32. High water level. 18. High hydrocarbon level. 41,43,55,57. Once the quality of the vacuum is satisfactory, the sputtering vessel is backfilled to 10-2 mbar with argon and sputtering is commenced. During the sputtering the quadrupole may be used to monitor water or hydrocarbons to ensure that they do not rise above critical levels and so degrade the quality of the sputtered film by converting the metal to the oxide form. With a fast response, short duration events such as burst of gas during valve operation may also be monitored. PLASMA ETCHING As with the sputtering process described above, there is an initial evacuation stage during which a quadrupole may be used to check for air leaks or contamination by unwanted species. Once the vacuum is satisfactory, the reactant gasses may be flowed through the system and the plasma struck. Mobile System The RGA, inlet valves and turbo pump would normally be attached directly to a spare port on the sputtering system. A flexible pipe would then be coupled to a backing pump. However the complete RGA, suplementry pumps and inlet valves can be incorporated into a mobile trolly. Connection to the Sputtering system is now through a detachable flexible stainless steel pipe and an isolation valve would be fitted at point A (figure1). The RGA system can now be easily moved from one sputtering system to another as the occasion demands. Represented by Larimax/ASI.. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. U.K. Tel: +44 (0) Fax: +44 (0) website http// sales@a-s-i.demon.co.uk Return to Index

31 Larimax Introducing COMPASS Gas Analysis System

32 COMPuter Assisted Spectrometry Systems - points the way for others to follow CONCEPT The COMPASS concept is to provide complete solutions to gas analysis problems. With a wide choice of inlet systems, vacuum systems, ion sources and flexible software, Compass can be easily configured to your application. Larimax AX600 SERIES MASS SPECTROMETER The heart of any compass is the mass spectrometer and the AX600 sets new standards in quadrupole anaysis. The outstanding performance capabilities of the AX600 are due to advances in both hardware and software made by ASI engineers over many years of research. It was necessary to address some fundamental weakness in conventional quadrupole design before achieving the objective - a new generation of high performance quadrupole mass analysers that could meet applications previously unattainable by such low cost instruments. There is not enough space in this leaflet to expand on all the unique features of the AX600 series and so a range of technical papers and application notes have been produced (see back page for details). ION SOURCES Open Ion Source This Ion source has been designed to minimise outgassing and to eliminate problems caused by background peaks. This has been achieved by the use of a lightweight open structure and reducing power dissipation. The need for high temperature bake-out of the vaccum system to reduce bakeground using ovens is completely eliminated. The open Ion Source is fitted with twin filaments. Both the filaments are easily rplacable by the user. 'NIBTRON'' Ion Source An importantant new development available as an option with the AX600 series mass spectrometers is the revolutionary 'NIBTRON ion source. This ion source completely eliminates any interfering background peaks and at the same time requires very little sample gas allowing much smaller samples to be analysed. This new ion source has made the former gas-tight (enclosed) ion source completely obsolete. AX600 SOFTWARE The AX600 is certainly the most advanced collection of low cost mass spectrometers, but they are also the easiest to use. Menu options are selected using mouse or keyboard control, and the mass spectrometer parameters are easily changed with a single button operation, and the computer does the rest. Mass spectrometer control is fully automatic, the operator using the keyboard or mouse to select the required precision first mass, scan width, Faraday or SEM detector, and the operation of the filament system. The screen displays are all in high resolution colour graphics and the comprehensive standard software suit will be augmented by additional upgrade kits which will be issued regulary to meet demand. Current software options include:- * Full and partial Spectrum display in Bargraph and analogue display modes. * 16 Channel Peak Select. * Multi-channel trend analysis Bargraph Display Multi-channel Trend Analysis Peak Select Mode Analogue Display Mode * Spectral storage and display. * Library storage/library search * Auto data logging. * Auto calibration routines. * Printer output. Selection of different Quadrupole Analyser Heads

33 INLET SYSTEMS In order to interface the low pressure requirement of the mass spectrometer to the environment of the 'real world' and hence cater for a wide range of analysis, Compass includes a choice of inlet systems from simple leak valves to computer controlled multi stream gas samplers. Many inlet systems are specifically designed to meet particular requirements and only a few of the more common ones are mentioned here. MEMBRANE INLETS A lot of interesting applications are being found for ASI membrane inlets. These inlet systems are thin teflon or silicon rubber membrane to separate a capillary inlet from the environment. Applications are as varied as the extraction of dissolved gases from fermentation broths to the sampling of atmospheres around chemical production plants. Larimax manufacture a range of different inlets to cater for different sample volumes. Bakeable versions are available to reduce memory effects for high accuracy analysis. VIAL INLETS This inlet is to analyse gas in small glass vials which are fitted with a septum. A special needle fitted to the end of a capillary inlet, pierces the septum and draws the enclosed gas through the capillary and into the mass spectrometer. A special valve arrangement stops air entering when the needle is extracted. This can also be adapted for other head space analysis in different types of packaging MULTI-STREAM GAS SAMPLING INLET Complete Gas Analysis System with Floor Standing Vacuum System CAPILLARY INLETS Capillary inlets, with and without bypass and with the option of electrical heaters to minimise condensation and memory effects and increase response times, can be an effective, low cost solution to interfacing sample areas to mass spectrometer analyser housing. BATCH INLETS Not all applications involve the analysis of a flowing stream of gas. Often a variable amount of gas sample is collected in a suitable container which then needs to be introduced to the mass spectrometer through a batch inlet system. The AX600 instrument is not expensive but we still accept that most users would prefer to introduce multiple samples into one mass spectrometer rather than buy a mass analyser for each sample stream. The multi stream gas sampling inlet allows the connection of up to 32 gas streams to one capillary inlet. Which is then used to introduce each selected sample into the source of the AX600. All streams not being sampled flow through their own individual inlet and outlet connections. Both the operation of electrical switching to select the channel (which can be one or more calibration gases) and determination of dwell time per channel can be under computer control. This inlet is very versatile but a typical application is for the sampling of dissolved gases (see membrane inlet) and off gases from multi-vessel fermentation and cell culture installations. DUAL Both high conductance and leak valves are provided to give inlet conditions selectable from atmosphere to high vacuum depending on requirements. This inlet is particulary useful for monitoring processes where vacuum conditions change during the course of the process, as happens in semiconductor production for instance. VACUUM SYSTEMS Compass vacuum systems are configured for each application. The selection of turbo molecular pump or diffusion pump, the optimum size of rotary pumps and control/monitoring equipment is made easier by relying on the wealth of experience of Larimax mass spectroscopist and vacuum engineers. In addition to the standard floor mounted and table top systems, Larimax have built small portable mass spectrometry systems for field operation where small size, light weight and low power requirements are of prime consideration.

34 E COMPASS FROM Larimax New Technology N Wide Range of Options W Ease of Use Solutions to Problems Larimax Compass are available for most gas analysis applications Residual Gas Analysis. Monitoring Semiconductor Manufacture. Environmental Pollution Monitoring. Leak Detection. Vacuum Furnaces. Vacuum Coating. Surface Science Reaction Kinetics. Electron Microscopes Medical Gas Analysis. Gas Permeation. Fermentation Gas Analysis. PRODUCT INFORMATION SHEETS AVAILABLE AX200 Series Mass Spectrometers. AX600 Series Mass Spectrometers. Dataquad Series Mass Spectrometers. Mass Spectrometer Software. Inlet Systems for Mass Spectrometers. The use of Compass for Environmental Monitoring. Continuous Monitoring in Biotechnology. Represented by: Larimax/ASI. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. Tel: +44 (0) Fax: +44 (0) website sales@a-s-i.demon.co.uk Return to Index

35 Larimax Introducing The TGA-1 Environmental Gas Analysis System

36 The TGA-1 -Trace Gas Analysis System for Environmental and Process Gas Monitoring. CONCEPT The TGA-1 is a fully integrated Computer controlled gas analysis system specifically designed and configured for Environmental monitoring of atmospheric gases and trace level detection of contaminants in process gases. The TGA-1 system incorporates the latest AX600 QMS system, membrane probe technology, with a powerful software package. Unlike other techniques the TGA-1 offers fast on line analysis with low ppb detection levels. Larimax AX600 SERIES MASS SPECTROMETER The heart of any compass is the mass spectrometer and the AX600 sets new standards in quadrupole analysis. The outstanding performance capabilities of the AX600 are due to advances in both hardware and software made by Larimax engineers over many years of research. It was necessary to address some fundamental weakness in conventional quadrupole design before achieving the objective - a new generation of high performance quadrupole mass analysers that could meet applications previously unattainable by such low cost instruments. Features. Low ppb detection of most hydrocarbons and organics Fully automated system for continuous on line measurements. Adjustable alarm level. Automatic data storage and retrieval. Automatic self-calibration. (against known calibration gas) Comprehensive software easily tailored to individual process requirements. Choice of vacuum systems. Choice of membrane probes for atmospheric or other process gas monitoring. Multi-valve inlet option for monitoring several separate gas streams. VACUUM SYSTEMS Our vacuum systems are configured for each application. The standard vacuum system consist of a turbo molecular pump backed by a 2 stage rotary pump fitted with oil mist filters. Penning and pirani gauges are available for control and monitoring of the vacuum system. These are interlocked with the mass spectrometer to provide fail safe operation during power failure and provide automatic start-up and resume normal operation when the power is returned. Complete Gas Analysis System with Floor Standing Vacuum System

37 INLET SYSTEMS In order to interface the low pressure requirement of the mass spectrometer to the environment of the 'real world' and hence cater for a wide range of analyses, the TGA-1 includes a choice of inlet systems from simple leak valves to computer controlled multi stream gas samplers. Many inlet systems are specifically designed to meet particular requirements and for trace level detection of hydrocarbons the membrane inlet is normally used. MEMBRANE INLETS A wide range of applications are being found for Larimax membrane inlets. Applications include environmental monitoring of the atmosphere, and process gas impurity measurements. These inlet systems use thin silicon rubber membrane to separate the Mass Spectrometer inlet from the environment. The process gas is usually pre-heated and the membrane probe can also temperature controlled to provide good stability. Membrane Inlet Waste Process Gas -> To Mass Spectrometer Ion Source MULTI-STREAM GAS SAMPLING INLET The AX600 instrument is not expensive but we still accept that most users would prefer to introduce multiple samples into one mass spectrometer rather than buy a mass analyser for each sample stream. The multi-stream gas sampling inlet allows the connection of up to 32 gas streams to one inlet system which is then used to introduce each selected sample into the source of the AX600. All streams not being sampled flow through their own individual inlet and outlet connections. Both the operation of electrical switching to select the channel (which can be one or more calibration gases) and determination of dwell time per channel can be under computer control. This inlet is very versatile but a typical application is for the sampling of dissolved gases (see membrane inlet) and off gases from multi-vessel fermentation and cell culture installations. AX600 SOFTWARE The AX600 is certainly the most advanced collection of low cost mass spectrometers, but they are also the easiest to use. Menu options are selected using mouse or keyboard control, and the mass spectrometer parameters are easily changed with a single button operation, and the computer does the rest. Mass spectrometer control is fully automatic, the operator using the keyboard or mouse to select the required precision first mass, scan width, Faraday or SEM detector, and the operation of the filament system. The screen displays are all in high resolution colour graphics and the comprehensive standard software suit will be augmented by additional upgrade kits which will be issued regularly to meet demand. Current software options include:- Full and partial Spectrum display in Bargraph and analogue display modes. 16 Channel Peak Select. Multi-channel trend analysis Spectral storage and display. Auto data logging. Auto calibration routines. Printer output. TGA-1 SOFTWARE Unlike other analytical techniques, the TGA-1, provides continuous online measurements every few seconds. Continuously stores the data. Provides easy retrieval of stored data that can be displayed in either trend mode against time or table format. The TGA-1 can also be set to carry out it's own fully automatic selfcalibration against a known reference gas. Alarm level can be pre-set over a wide range, and will provide visual indication in the event that monitored gases exceed the alarm level. An additional feature of the software provides muti-channel averaging which can give further improved detection levels when the instrument is used in 'single gas monitoring mode'. The multvalve inlet option allows up to 32 separate gas streams to be connected to the TGA-1 for automatic sequential analysis.

38 TGA-1 SYSTEMS FROM LARIMAX. Detection Levels achieved Acetone Petrol Trichloroethylene Cyclohexane Benzene Toluene Xylene IN WATER 10ppb 1ppb 5ppb 1ppb 6ppb 4ppb 3ppb IN AIR 1ppb 0.2ppb 0.6ppb 0.2ppb 0.5ppb 0.3ppb 0.2ppb IN CO2 Process Gas 3ppb 2ppb 2ppb Larimax. Systems are available for most gas analysis applications Residual Gas Analysis. Monitoring Semiconductor Manufacture. Environmental Pollution Monitoring. Leak Detection. Vacuum Furnaces. Vacuum Coating. Surface Science Reaction Kinetics. Electron Microscopes Medical Gas Analysis. Gas Permeation. Fermentation Gas Analysis. PRODUCT INFORMATION SHEETS AVAILABLE AX600 Series Mass Spectrometers. AX200 Series Mass Spectrometers. Dataquad Series Mass Spectrometers. Mass Spectrometer Software. Inlet Systems for Mass Spectrometers. Continuous Monitoring in Biotechnology. Represented by: Larimax/A.S.I. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. Tel: +44 (0) Fax: +44 (0) website sales@a-s-i.demon.co.uk Return to Index

39 Larimax Introducing BioQuad Fermentation Gas Analysis System Complete Gas Analysis System with Floor Standing Vacuum System

40 Features. Fully automated system for continuous on line measurements. Automatic data storage and retrieval. Automatic self-calibration. Comprehensive software easily tailored to individual process requirements. Choice of vacuum systems. Multi-valve inlet option for monitoring several Fermentation Vessels. Adjustable alarm level. Choice of membrane probes for analysis of dissolved species. Carbon Evolution Rate (CER), Oxygen Uptake Rate (OUR) and Respiratory Quotient (Rq) automatically calculated and displayed. CONCEPT The Bio-Quad is a fully integrated Computer controlled gas analysis system specifically designed and configured for gas analysis for fermentation and cell culture. The Bio-Quad system incorporates the latest AX600 QMS system with a powerful software package. A Choice of multi-valve inlet systems for online analysis of up to 16 fermentation vessels. And a choice of optional membrane probes for the analysis of dissolved gases. A.S.I. AX600 SERIES MASS SPECTROMETER The heart of any system is the mass spectrometer and the AX600 sets new standards in quadrupole analysis. The outstanding performance capabilities of the AX600 are due to advances in both hardware and software made by ASI engineers over many years of research. It was necessary to address some fundamental weakness in conventional quadrupole design before achieving the objective-anew generation of high performance quadrupole mass analysers that could meet applications previously unattainable by such low cost instruments. VACUUM SYSTEMS Our vacuum systems are configured for each application. The standard vacuum system consist of a turbo molecular pump backed by a 2 stage rotary pump fitted with oil mist filters. Penning and pirani gauges are fitted for control and monitoring of the vacuum system. These are interlocked with the mass spectrometer to provide fail safe operation during power failure and provide automatic start-up and resume normal operation when the power is returned. MULTI-STREAM GAS The AX600 instrument is not expensive but we still accept that most users would prefer to introduce multiple samples into one mass spectrometer rather than buy a mass analyser for each sample stream. The multi-stream gas sampling inlet allows the connection of up to 32 gas streams to one inlet system which is then used to introduce each selected sample into the source of the AX600. All streams not being sampled flow through their own individual inlet and outlet connections. Both the operation of electrical switching to select the channel (which can be one or more calibration gases) and determination of dwell time per channel can be under computer control. This inlet is very versatile but a typical application is for the sampling of dissolved gases (see membrane inlet) and off gases from multi-vessel fermentation and cell culture installations.

41 Bio-Quad. - Gas Analysis System for Fermentation and Process Gas Monitoring. INLET SYSTEMS In order to interface the low pressure requirement of the mass spectrometer to the environment of the 'real world' and hence cater for a wide range of analysis, the Bio-Quad includes a choice of inlet systems from simple leak valves to computer controlled multi stream gas samplers. Many inlet systems are specifically designed to meet particular requirements and for fermentation applications the capillary inlet is normally used. MEMBRANE INLETS The bio-quad not only offers a tremendous flexibility in the monitoring of multiple off gas streams but can also be supplied with a membrane probe to allow the analysis of gases and volatiles extracted directly from the fermentation broth. These inlet systems use thin silicon rubber or Teflon membrane to separate the Mass Spectrometer inlet from the broth. The gases which permeate through the membrane are taken to the mass spectrometer analyser by a carrier gas. This technique allows multiple probes to be used with the multichannel inlet system as for off gas analysis. Figure 1. Carrier Gas In Membrane Inlet of Mass Spectrometer Membrane Probe Liquid AX600 SOFTWARE The AX600 is certainly the most advanced collection of low cost mass spectrometers, but they are also the easiest to use. Menu options are selected using mouse or keyboard control, and the mass spectrometer parameters are easily changed with a single button operation, and the computer does the rest. Mass spectrometer control is fully automatic, the operator using the keyboard or mouse to select the required precision first mass, scan width, Faraday or SEM detector, and the operation of the filament system. The screen displays are all in high resolution colour graphics and the comprehensive standard software suit will be augmented by additional upgrade kits which will be issued regularly to meet demand. Current software options include:- BIOQUAD SOFTWARE Unlike other analytical techniques, the Bio-Quad, provides continuous online measurements every few seconds. Continuously stores the data. Provides easy retrieval of stored data that can be displayed in either trend mode against time or table format. The Bio-Quad can also be set to carry out it's own fully automatic self- calibration against a known reference gas. Alarm level can be pre-set over a wide range, and will provide visual indication in the event that monitored gases exceed the alarm level. By continuous monitoring of both the inlet and outlet streams of a bio-reactor the software can automatically calculate and display the carbon evolution rate (CER), Oxygen uptake rate (OUR) and the Respiratory Quotient (Rq). This data can be automatically stored to disc if required. The mult-valve inlet option allows up to 32 separate gas streams to be connected to the Bio-Quad for automatic sequential analysis.

42 BioQuad From Larimax There are two important derivatives obtained from continuous monitoring of the oxygen and carbon dioxide levels on inlet and outlet streams. The first is the Respiratory Quotient (Rq) and the second is the Oxygen Uptake Rate (OUR). Both give good status reports on the amount of biomass present and if growth is positive or negative. The Respiratory Quotient is the ratio between the increase in carbon dioxide level against the reduction in oxygen, and the Oxygen Uptake Rate is the reduction in oxygen level with respect to time. During some plant cell cultivations, the mass spectrometer can be used to monitor the nitrogen levels on the inlet and exhaust lines so as to identify the amount of nitrogen fixation taking place. In all applications it is possible to include measurements of the four main air gases, nitrogen, oxygen, argon, and carbon dioxide on both sides of the bioreator so as to achieve a so called mass balance and check the accuracy of results. Larimax Systems are available for most gas analysis applications Residual Gas Analysis. Monitoring Semiconductor Manufacture. Environmental Pollution Monitoring. Leak Detection. Vacuum Furnaces. Vacuum Coating. Surface Science Reaction Kinetics. Electron Microscopes Medical Gas Analysis. Gas Permeation. Fermentation Gas Analysis. PRODUCT INFORMATION SHEETS AVAILABLE AX200 Series Mass Spectrometers AX600 Series Mass Spectrometers. Dataquad Series Mass Spectrometers. Mass Spectrometer Software. Inlet Systems for Mass Spectrometers. Environmental and Process Gas Analysis System. Compass Gas Analysis System. Represented by: A.S.I. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon EX38 7HP. Tel: +44 (0) Fax: website sales@a-s-i.demon.co.uk Return to Index

43 Ion Source Options. All electron impact ion sources manufactured by ASI/Larimax are fitted with 2 individually replaceable filaments. This has the advantage that in the event of a filament failure the faulty filament can be replaced at a convenient time so a spare is always available for back-up. Most of our competitors have a twin filament assembly (Both filaments mounted on the same plate). This has the disadvantage that in the event of a filament failure the user has to run without a backup until the second filament fails or replace both filaments together Open Ion Source The open ion source is of radial symmetric design and is fitted as standard on all Larimax quadrupole analysers. This source is suitable for both Residual gas Analysis and Gas Analysis applications. Axial Beam Source. The axial beam source is suitable for molecular beams or ion beams that are parallel to the quadrupole axis. A clear aperture of 4mm exist through the center of the source. The two filaments are mounted on the side of the source to enable the source to be positioned close to the exit point of the ion/molecular beam. Cross Beam Source. The cross beam source is suitable for molecular beams or ion beams that are at right angles to the quadrupole axis. A clear aperture of 4 mm. exist through the side of the source. This source is usually chosen when the beam may contain condensable vapours that may contaminate the quadrupole. A cold finger may be positioned on the other side of the source to trap condensable vapours.

44 Larimax NIBTRON ION SOURCE. (SUPPRESSED BACKGROUND) A major breakthrough in quadrupole mass spectrometry has recently been achieved by A.S.I. with the introduction of the new NIBTRON ion source. This new Ion Source is available as an option, on the ASI quadrupole gas analysis systems and provides the following advantages and unique features:- 1) Elimination of 99.9% or more of the interfering background peaks. 2) Provides greatly improved accuracy and performance. 3) Allows much simpler, lower pumping speeds, and hence much lower cost vacuum systems. 4) Eliminates the need for bake-out ovens. 5) Allows much smaller gas samples to be measured. 6) Reduces memory effects from previous gas samples 7) Eliminates catalytic reactions from the hot filament being measured. CONVENTIONAL ION SOURCES. Ionise both the sample gas and the residual gases present in the vacuum system. These residual background peaks often make gas analysis very difficult. To reduce these background peaks to acceptable levels it is essential to frequently bake the vacuum system to high temperature. Even after bake out, residual peaks are still present, limiting the accuracy to which gas analysis can be achieved. These residual peaks will subsequently increase in amplitude when sample gas is introduced into the vacuum chamber due to desoption from the chamber walls, making it difficult to determine the percentage of sample peak that may be present in a changing background. NIBTRON. The new NIBTRON quadrupole analyser has an extremely low sensitivity to residual gas ions, whilst at the same time has a high sensitivity to sample gas ions. This improvement in ionisation ratio is in excess of 2000, producing clean sample gas spectra even under poor vacuum/high background conditions. This is illustrated below. Comparison is made between a q.m.s. analyser fitted with a conventional ion source and a NIBTRON analyser. These comparisons were made under identical vacuum conditions. The test were carried out on a freshly pumped vacuum chamber whilst the residual gases were still at a high level. The system pressure was at 3 x 10-6 mbar. A leak valve was then opened, admitting an air sample, increasing the pressure by 1 x 10-6mBar. The following two scans were made using a DQC2000 mass spectrometer and cover the mass range from approx amu. CONVENTIONAL SOURCE. The background pressure is 3x10e-6 mbar and the air sample pressure is 1x10e-6 mbar. The very high level of background peaks make it difficult to measure the argon or CO2 peaks from an Air sample. The mass 40 peak is mainly background and the CO2 peak at mass 44 is completely masked by the high background of CO2 produced mainly from the filament. NIBTRON SOURCE. The same background conditions as above. The background pressure is 3 x 10e-6 mbar and the air sample pressure is 1x10e-6 mbar. NOTE.- the complete absence of residual background peaks Masses 32, 33, 34=Atmosheric oxygen and isotopes. Mass 40= Atmosheric Argon. 10xFSD Mass 44 Atmosheric CO2. Approx 330ppm. Note.- The higher sample peak heights are due to the high sensitivity of the NIBTRON Source. Note:- Because of its very low sensitivity to residual gases, the NIBTRON is totally unsuitable for RGA applications. Anglo Scientific Instruments. 3 Devon Units, Hatchmoor Industrial Estate, Torrington, Devon, EX38 7HP. U.K. Tel/Fax: +44 (0) sales@a-s-i.demon.co.uk Website http//a-s-i.demon.co.uk

45 Spares Filaments Spare filaments for Analysers are individually replaceable. Tungsten filaments are normally supplied in packs of 4 and Thoria coated filaments are supplied in packs of 2. Technical Notes. Which Filament? The majority of our competitors use a twin filament assembly. That means that when one of the filaments blows the customer has a difficult decision. Does he replace the filament assembly throwing the remaining good filament away, or does he run on the second filament and hope it does not blow during a critical measurement when there is no back-up. All ASI/Larimax RGA's are fitted with two filaments. The filaments are individually replaceable. Therefore if one filament blows, that filament can be changed at a convenient time. And the other good filament remains on the analyser. Tungsten Filaments. Operating temperature for Pure Tungsten approx 2200C available for Dataquad/Selectorr/DQC2000/HPQ instruments. Operating temperature for Thoriated Tungsten (1% Thoria) approx 1950C (AX200 and AX600 instrument only) A good low cost general purpose filament. Under high vacuum, below 10e-6mBar filaments will last many months and sometimes many years. Can be used at high pressure in inert atmospheres. Can be used in Hydrogen or reducing atmospheres. Safe to handle filaments. Disadvantages Life is reduced in oxidising atmospheres above 5x 10e-6mBar Life is reduced in high partial pressures of water vapour (10e-5mBar) due to filament erosion. Sudden exposure to high pressure above 10-2mBar of oxidising atmosphere can cause instant oxidation and burn out of filament. Will burn out instantly if switched on at atmospheric pressure. Tungsten filaments usually produce background peaks at mass 28 (CO) and 44(CO2). Can produce a catalytic action with some chemicals. Comments:- Slow evaporation of filament will cause the filament to become thinner over a very long period of time, with a reduction of operating current eventually leading to failure. Normally recommended in medium and high vacuum systems for general-purpose residual gas analysis. Continued Overleaf

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